الفهرس 
Advanced Analytical Techniques for Screening and Determination of Some Residues and Contaminants in Functional Foods
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Abstract
Functional foods provide nutritional and health benefits, yet they could be contaminated with residues like pesticides and polychlorobiphenyls. These residues affect the safety, quality, and consequently the commercial value of functional foods. Therefore, the validity and efficiency of residue determination methods constitute a major analytical concern. Reduction of matrix effect (ME) has always been the golden key for guaranteed sensitivity, selectivity, and high throughput analysis. This study aims for accurate determination and streamlined quantification of 200 pesticide residues in 16 matrices. Hence, a modified QuEChERS extraction protocol coupled to GC-MS/MS was then employed and separations were obtained in 25 min. Dilution of the final extracts of fresh and herbal samples was carried out to achieve an acceptable balance between sensitivity and peak characteristics. Dilution factors of 1x and 5x were selected for fresh and herbal samples, respectively. Principal component analysis (PCA) was then independently applied on the digitally exported total ion chromatograms (TICs) of the studied matrices and the calculated ME%. PCA score/loading plots of TICs demonstrated the key matrix constituents that influenced the obtained trends. Similarly, three main clusters were obtained after PCA of ME% indicating a dependent relationship between matrix type and the obtained effects. Out of the obtained three clusters, an appropriate representative matrix-matched calibration (R-MMC) was selected for ME compensation. Based on the EU validation guidelines, the proposed protocol was validated at 2 and 10 μg/Kg with acceptable method performance. Four proficiency testing (PT) and commercial samples were successfully analyzed. The proposed protocol would help laboratories to increase sample processing capacity and to ensure the safety of functional food products. This work should serve in setting standards that warranty the quality/safety of functional foods by national regulatory authorities.
On the other hand, Infant formulae (IF) are a significant category of special foods designed to replace a mother’s breast milk. In this regard, IF quality and safety testing is critical to ensuring the health and development of this high-risk, vulnerable group. This study aims to develop and validate a streamlined assay protocol for water-soluble vitamins, vitamin D3, and some unauthorized antibacterial residues from various chemical classes. Hence, different IF compositions (cow and goat milk-based formulae) were extracted using an acetonitrile, water, and methanol (3:4:3 v/v/v) mixture. Following that, the compounds were determined using a direct injection into an ultra-sensitive LC-MS/MS. Separations were carried out in a single chromatographic run over 12.0 minutes, using a Poroshell 120 EC-C18 column. Gradient elution was carried out with a buffered mobile phase of 10 mMole ammonium formate and methanol. The performance characteristics of the method were tested and validated in accordance with EU validation guidelines 808/2021/EC, 657/2002/EC, and Eurachem/CITAC. For all analytes, decision limits (CCα) and detection capabilities (CCβ) as well as LODs and LOQs were well below the RPA of chloramphenicol (0.15 μg/kg) and the lowest achieved calibration levels (LCLs) per each studied compound. The LODs, LOQs, R2, CCα, CCβ, percentage recovery, and CV% ranges were (0.0001-0.104 µg/mL, and 0.002-2.36 ng/mL), (0.00004-0.342 µg/mL, and 0.005-7.78 ng/mL), ≥ 0.990, (0.02-10.29 µg/Kg), (0.04-17.48 µg/Kg), (85.4-110.3%), and (0.8-19.3%), respectively. The reliability of the proposed assay was successfully attested through its application to thirty domestic commercial IF samples from global manufacturers as well as two previously analyzed PT samples. The results confirmed the practicality of the assay along with the suitability of the surveyed samples for infant consumption. This protocol would assist Egyptian regulatory authorities in making the proper decisions regarding the quality and safety of IF shipments while maintaining the least amount of disruption to the stream of commerce.